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61.
L.M. León M.C. Gonzalez J.R. Quintana F. Zamora Armando Martinez G.M. Guzman 《European Polymer Journal》1982,18(3):229-231
The Ptitsyn-Eizner λ flexibility parameter for poly(N-vinylcarbozole) solutions under theta conditions has been found to be 6.31, demonstrating the rigidity imparted to the polymer chain by the carbazole group. A study has been made of the variation of this parameter with solvent and temperature. A study has been made of the variation of λ in a conformational transition of poly(methyl methacrylate). 相似文献
62.
The synthesis of the new esterglycidyl compounds produced by condensation of bis-carboxyimides with a large excess of epichlorohydrin were reported. To define the optimal conditions of condensation the process with monofunctional compounds were studied at first. For all synthesis, yield and epoxide and chlorine contents were found. The structure of glycidyl esters was determined by elementary analysis, IR and 1H and 13C NMR spectra. The physical properties were also defined. 相似文献
63.
Simplified procedures for the analysis of polycyclic aromatic hydrocarbons in water, sediments and mussels 总被引:9,自引:0,他引:9
We describe in this paper simple and robust analytical protocols to determine the 16 polycyclic aromatic hydrocarbons (PAHs) of the US Environmental Protection Agency priority list in water, sediment and mussels. For water samples, eight different solid-phase extraction (SPE) sorbents have been compared and among them, C18 provided highest recoveries and limits of detection of 0.3-15 ng/L. For lyophilized sediments, Soxhlet and ultrasonic extraction were compared, and the last one permitted to recover all analytes with highest repetitivity and was validated by analysing a certified reference material. Finally, the analysis of mussels was undertaken using Soxhlet, ultrasonic and pressurized liquid extraction (PLE) and the performance of several clean-up steps are compared. Whereas for the former two, incomplete recovery or losses of some analytes were evidenced, PLE permitted a more efficient extraction and although alkaline digestion was necessary to remove coextracted compounds, the method gave acceptable recoveries and limits of detection of 0.5-7.7 microg/kg dry mass, as for sediments. In all cases, analysis was performed by gas chromatography coupled to mass spectrometry and internal standard quantification was performed using five deuterated PAHs. Each method performance is discussed for the three matrices analysed and the paper reports advantages and disadvantages of each for their routine application in monitoring programs. 相似文献
64.
Attachment of an amino acid to a solid support by its side chain is sometimes necessary to take advantage of an alpha-carboxylic group available for diverse modifications, including the incorporation of a fluorophore for the preparation of fluorogenic substrates. In contrast to most other amino acids, anchoring the guanidinium group of an arginine to a resin requires the use of a supplementary linker. To avoid the usually multistep synthesis of such a linker as well as its difficult attachment to the guanidine group, we developed a simple method where the guanidine group is built on a Rink amide resin. Our strategy followed the steps of guanidine formation: (i) addition of an isothiocyanate derivative of ornithine to the amino group of a solid support, yielding Nomega-linked thiocitrulline; (ii) S-methylation of thiourea; (iii) guanidinylation using ammonium acetate. Cleavage of the resin generated the arginine-containing compound, the amine group of the resin becoming part of the guanidine. We have demonstrated the usefulness of this method by the synthesis of a series of fluorogenic substrates for trypsin-like serine proteases, which were obtained in high yield and purity. Then, our strategy also allowed generation from the same precursor differentially substituted arginine derivatives, including Nomega-methyl- and Nomega-ethylarginines. The ability to prepare such analogues together with the intermediates thiocitrulline and S-methylisothiocitrulline from a unique precursor while the alpha-amine and carboxylic groups remain available for modification also makes this method a powerful tool for combinatorial solid-phase synthesis of NO synthase inhibitors. 相似文献
65.
F. Bosch Reig V. Peris Martinez F. Bosch Mossi J. V. Gimeno Adelantado 《Fresenius' Journal of Analytical Chemistry》1992,342(4-5):295-298
Summary An algorithm for quantifying interelemental effects in X-ray fluorescence techniques is developed. By applying an addition process, the ratio between the mass absorption coefficients of the analyte and the unknown sample (
i
*
/
s
*
) is calculated to correct the fluorescence intensity of the element to be determined and linearize the I-c calibration plot. This coefficient can be calculated graphically and numerically. The method is applied to the determination of tin in lead alloys with good results over wide concentration ranges.Notation used Q
Constant of proportionality in Eq. (4)
X-ray fluorescence intensity of the I
i
o
standard
- I
i
s
unknown sample
- I
i
ns
dilute unknown sample
- I
i
ms
unknown sample after addition of i analyte
Corrected fluorescence intensity of the I
i
cs
unknown sample
- I
i
msc
unknown sample after addition of i analyte
Relationship of fluorescence intensity between Ri
sample and standard
- R
i
dilute sample and standard
Factor of fm
addition
- fx
addition equivalent to the mass fraction of the i analyte in the unknown sample
Mass absorption coefficient of
i
*
analyte
-
s
*
unknown sample
-
ms
*
unknown sample after addition
Mass fraction of c
i
s
analyte
- c
i
ms
unknown sample after addition 相似文献
66.
The method for analysis of inorganic cations in brine solutions was developed. Ion chromatography is a well-established and accepted technique in the determination of a variety of inorganic ions. However, there are significant complications when ion chromatography is used to determine trace concentrations of inorganic ions in brine matrices. The brine solution in our study was made to simulate the solution from the Waste Isolation Pilot Plant. Instrumental parameters such as eluent composition, flow-rates, and sample loop volumes were investigated to arrive at the optimum condition for the determination of the cations with minimal dilution. Separation was carried out in a Dionex CG12A/CS12A with 8.25 mM H2SO4 as eluent at 1.2 ml/min flow-rate. Our results indicated that ion chromatography is an accurate and a good alternative method for the analysis of cations in brine solution. 相似文献
67.
R. Alan Jones Pilar Martinez Fresneda Teresa Aznar Saliente José Sepúlveda Arques 《Tetrahedron》1984,40(23):4837-4842
The overall rates of reaction of 1-substltuted-1- (1-methyl-2-indolyl)ethenes with dimethyl acetylenedicarboxylate are considerably lower than those of the corresponding 2-vinyl- pyrroles. Steric interaction between the N-methyl group on the indole ring and the 1-substituent on the ethenyl group prevents the diene system adopting a coplanar configuration and, thereby, inhibits the π4 + π2 cycloaddition reaction of the system with dimethyl acetylenedicarboxylate. Under such conditions, the indolylethene preferentially undergoes a Michael addition reaction at the 3-position. The π4 + π2 cycloaddition reaction is promoted at elevated temperatures. No evidence was found for a Cope rearrangement of the Michael adducts to give the dihydrocarbazole. 相似文献
68.
William Clegg Todd B. Marder Sylvain Nlate Andrew J. Scott 《Acta Crystallographica. Section C, Structural Chemistry》2007,63(10):o603-o605
The title compound, C36H26B4F24N2O6·0.667C4H10O, has centrosymmetric tetraboradioxane molecules, half each of three of these comprising the asymmetric unit together with a molecule of diethyl ether. Disorder affects most of the CF3 groups and one ethyl group of the solvent molecule. The B4O2 rings are approximately planar and contain two B atoms with trigonal geometry and two with distorted tetrahedral geometry, the B—O bonds for the four‐coordinate B atoms being longer than those for the three‐coordinate B atoms. N—H...O hydrogen bonds link two of the crystallographically independent molecules together in chains, while the third molecule forms discrete trimolecular clusters with two solvent molecules via N—H...O hydrogen bonds. This is the first crystallographically characterized example of a tetrabora‐dioxane molecule containing both four‐ and three‐coordinate B atoms. 相似文献
69.
Klimova-Berestneva T. Martinez Garcia M. Meleshonkova N. N. Klimova E. I. 《Russian Journal of General Chemistry》2001,71(10):1626-1631
The asymmetric induction in the synthesis of 3,4,5-trisubstituted 4,5-dihydropyrazoles with ferrocenyl substituents, starting from the E and Z isomers of ,-unsaturated ketones was studied. A high diastereoselectivity was revealed at the 1,2 chiral center chiral center induction, which is independent of the configuration of the starting chalcones. 相似文献
70.
Bustamante JJ Garcia M Gonzalez L Garcia J Flores R Aguilar RM Trevino A Benavides L Martinez AO Haro LS 《Electrophoresis》2005,26(23):4389-4395
A method for separating proteins with a molecular mass difference of 2 kDa using SDS-PAGE under nonreducing conditions is presented. A sample mixture containing several human growth hormone (hGH) isoforms was initially separated on a weak anion-exchange column. Fractions rich in 24 kDa hGH as determined by analytical SDS-PAGE were pooled and further separated by cation-exchange chromatography. The fractions pooled from the cation-exchange chromatography contained two hGH isoforms with a 2 kDa molecular mass difference according to SDS-PAGE analysis, 22 and 24 kDa hGH. The 22 and 24 kDa hGH were separated using continuous-elution preparative double-inverted gradient PAGE (PDG-PAGE) under nonreducing conditions. The preparative electrophoresis gel was composed of three stacked tubular polyacrylamide matrices, a 4% stacking gel, a 13-18% linear gradient gel, and a 15-10% linear inverted gradient gel. Fractions containing purified 24 kDa hGH were pooled and Western blot analysis displayed immunoreactivity to antihGH antibodies. PDG-PAGE provides researchers with an electrophoretic technique to preparatively purify proteins under nonreducing conditions with molecular mass differences of 2 kDa. 相似文献